Abstract: In order to obtain accurate and high-resolution X-ray photoelectron spectroscopic (XPS) data, different sample preparation methods were used to study the XPS testing results of different types of conductive powders, non-conductive powders and mixed powders. The effect of different sample preparation methods on testing results were discussed from the aspects of half-peak width, charge, authenticity, sample preparation efficiency and data processing. The results showed that the adhesive sample preparation was better than the indium chip sample preparation for conductive powders and non-conductive powders, and the carbon conductive tape was better. For mixed samples, the results of Scotch double-sided tape were better than those of the other three sample preparation methods. In addition, the indium chip sample preparation can be used as a reference method for the charge correction in data processing.